9 - STEP 2...

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STEP 2: 3-METHOXY-1,3,5(10),8(9),14(15)-ESTRAPENTAENE-17-ONE CH 3 O CH 3 O CH 3 O OH CH 3 O O + HOAc, xylenes 1. Procedure You will do this step TWO times, the first time on a small scale using ~250 mg of material. After learning which spot is your product from NMR analysis of various fractions isolated during column chromatography of the product mixture from the small- scale reaction, you will bring the rest of your material through in the second reaction. Dissolve the crude 1-hydroxy-1-vinyl-6-methoxy tetralin (1.00 equiv) prepared in the previous experiment in xylenes (sol’n ~ 0.80 M) in a three-necked round-bottomed flask equipped with a reflux condenser in the center neck, a magnetic stirbar, and two rubber septa (Figure 2). Add 2-methyl-1,3-cyclopentanedione (1.01 equiv) and glacial acetic acid (10 equiv) to the reaction solution (note 1). Flush the apparatus with nitrogen, then affix a septum and a nitrogen balloon to the top of the reflux condenser. Heat the reaction mixture to reflux using an oil bath or a heating mantle as a heat source (note 2).
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